CN103771517A - Method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets - Google Patents
Method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets Download PDFInfo
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- CN103771517A CN103771517A CN201410022747.7A CN201410022747A CN103771517A CN 103771517 A CN103771517 A CN 103771517A CN 201410022747 A CN201410022747 A CN 201410022747A CN 103771517 A CN103771517 A CN 103771517A
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Abstract
The invention discloses a method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets and relates to a method for preparing two-dimensional MoS2 nanosheets. The problems that the existing process for preparing the MoS2 nanosheets is complex, the thickness of the obtained MoS2 nanosheets are not close enough to a single layer and the concentration of the MoS2 nanosheets in suspension is low are solved. The preparation method comprises the following steps: 1, mixing MoS2 block powder with a dispersing solvent, thereby obtaining initial mixed liquor; 2, shearing the initial mixed liquor at a high speed; 3, performing ultrasonic treatment on the mixed liquor; 4, finally performing centrifugal treatment on the mixed liquor, standing, taking the supernatant, and obtaining the two-dimensional MoS2 nanosheet suspension. The process is simple and feasible, the fluorescence phenomenon of the obtained MoS2 nanosheet suspension is obviously enhanced, the thickness of the MoS2 nanosheets is closer to the single layer, and the concentration of the nanosheets is higher. The method is mainly applied to the fields of semiconductors, optoelectronic devices, aerospace, nondestructive testing and composite materials.
Description
Technical field
The present invention relates to a kind of two-dimentional MoS
2the preparation method of nanometer sheet.
Background technology
Two-dimensional nano sheet (2D-nanasheets) is the thinnest a kind of function nano material, and it has the thickness of atom or molecule and infinitely-great planar dimension compared with thickness.MoS
2in layer, be a kind of S-Mo-S stacking,vertical structure, interlayer is with faint Van der Waals force combination.Just because of this special structure makes to destroy MoS
2interlaminar action, prepare the MoS of individual layer
2nanometer sheet becomes possibility.The MoS of individual layer
2thickness is about
block MoS
2be that band gap width is the indirect band-gap semiconductor of 1.2eV, its fluorescence (PL) signal is very weak.But the MoS of individual layer
2be direct band-gap semicondictor, its energy gap is 1.9eV, has very strong PL signal.The change of this character makes MoS
2nanometer sheet can produce some special reactions to electricity, magnetic, light etc.Theoretical and experiment report shows MoS simultaneously
2band gap width with STRESS VARIATION, PL peak can be with STRESS VARIATION.This makes it have huge application prospect at semiconductor applications.In addition, MoS
2" dangling bonds " and its excellent thermostability and mechanical property all make to there is application potential more widely.MoS
2nanometer sheet is described as semiconductor applications " Graphene ", and it will will show very large application prospect aspect opto-electronic device and strongthener multi-functional.
At present, obtain individual layer MoS
2the method of nanometer sheet mainly contains micromechanics method, ion graft process, reactive deposition method, solvent-thermal method etc.Micromechanics method is prepared MoS by mechanically peel
2nanometer sheet, the MoS that this legal system is standby
2nanometer sheet comparatively small amt, can not widespread use actual production.The complicated process of preparation of ion graft process is high to preparation environmental requirement.The MoS that reactive deposition legal system is standby
2nanometer sheet is second-rate.Solvent-thermal method is at preparation MoS
2nanometer sheet complex process, need to add tensio-active agent, easily introduces impurity.Ultrasonic dispersion is the MoS preparing preferably at present
2the method of nanometer sheet suspension, this method technical process is simple and easy to do, MoS
2nanometer sheet suspension also has more practical use.But prepare MoS by ultrasonic dispersion
2the concentration of nanometer sheet suspension is less, MoS
2the thickness low LCL of nanometer sheet approaches individual layer.In addition, the preparation technology of ultrasonic dispersion neither be very perfect and unified, need to constantly improve and optimize.
Summary of the invention
The present invention seeks in order to solve existing preparation MoS
2the complex process of nanometer sheet, the nanometer sheet thickness low LCL obtaining approaches individual layer and MoS
2moS in nanometer sheet suspension
2the problem that nanometer sheet concentration is less, and a kind of two-dimentional MoS disperseing based on liquid phase is provided
2the preparation method of nanometer sheet.
The present invention is based on the two-dimentional MoS that liquid phase is disperseed
2the preparation method of nanometer sheet follows these steps to realize:
One, by the MoS of natural hexagonal structure
2bulk powder is mixed with dispersion solvent, preparation MoS
2initial mixing liquid;
Two, adopt high speed shear emulsification instrument, with the shearing rate of 10000rpm～20000rpm, the initial mixing liquid of step 1 is carried out to high speed shear 20min～100min, obtain the mixed solution after shearing treatment;
Three, the mixed solution after shearing treatment step 2 being obtained carries out supersound process, obtains the mixed solution after supersound process;
Four, the mixed solution after the supersound process with the rotating speed of 1500rpm～6000rpm, step 3 being obtained carries out centrifugal treating, after centrifugal completing, gets supernatant liquid, leaves standstill 22～26h, and then gets the supernatant liquid of the reaction solution having left standstill, and obtains two-dimentional MoS
2nanometer sheet suspension;
Wherein the dispersion solvent described in step 1 is 1-Methyl-2-Pyrrolidone (NMP), l-vinyl-2-pyrrolidone (NVP), dimethyl sulfoxide (DMSO) (DMSO) or dimethyl formamide (DMF).
The present invention is based on the two-dimentional MoS that liquid phase is disperseed
2the preparation method of nanometer sheet mainly comprises following advantage:
1, the present invention prepares two-dimentional MoS
2the technological operation of nanometer sheet suspension is simple, and equipment used is this area conventional instrument, and process cycle is short, lower to the requirement of process environments, with low cost.
2, the MoS of preparation
2the concentration of nanometer sheet suspension is large, output is high, good stability.Contrast known MoS
2the fluorescence phenomenon of nanometer sheet suspension obviously strengthens, MoS
2nanometer sheet thickness is about 2nm left and right, and the number of plies is approximately 1～2 layer, MoS
2the thickness of nanometer sheet more approaches individual layer.
3, the MoS of preparation
2nanometer sheet suspension is selected common solvent, without adding the easily liquid of generation impurity such as tensio-active agent or intercalator, the two-dimentional MoS of preparation
2the purity of nanometer sheet suspension is high, and quality is good.The present invention is mainly used in semi-conductor, opto-electronic device, aerospace, nondestructive testing and prepare composite.
Accompanying drawing explanation
Fig. 1 is MoS prepared by embodiment mono-
2moS in nanometer sheet suspension
2the afm image of nanometer sheet;
Fig. 2 is the gauge figure of the partial cross section that cuts in Fig. 1;
Fig. 3 is MoS prepared by embodiment mono-
2the fluorescence spectrum figure of nanometer sheet suspension.
Embodiment
Embodiment one: the two-dimentional MoS that present embodiment is disperseed based on liquid phase
2the preparation method of nanometer sheet follows these steps to implement:
One, by the MoS of natural hexagonal structure
2bulk powder is mixed with dispersion solvent, preparation MoS
2initial mixing liquid;
Two, adopt high speed shear emulsification instrument, with the shearing rate of 10000rpm～20000rpm, the initial mixing liquid of step 1 is carried out to high speed shear 20min～100min, obtain the mixed solution after shearing treatment;
Three, the mixed solution after shearing treatment step 2 being obtained carries out supersound process, obtains the mixed solution after supersound process;
Four, the mixed solution after the supersound process with the rotating speed of 1500rpm～6000rpm, step 3 being obtained carries out centrifugal treating, after centrifugal completing, gets supernatant liquid, leaves standstill 22～26h, and then gets the supernatant liquid of the reaction solution having left standstill, and obtains two-dimentional MoS
2nanometer sheet suspension;
Wherein the dispersion solvent described in step 1 is 1-Methyl-2-Pyrrolidone (NMP), l-vinyl-2-pyrrolidone (NVP), dimethyl sulfoxide (DMSO) (DMSO) or dimethyl formamide (DMF).
The MoS of the natural hexagonal structure that present embodiment step 1 is used
2bulk powder is by commercially available.
The two-dimentional MoS that present embodiment is disperseed based on liquid phase
2the preparation method of nanometer sheet utilizes specific intensive polar solvent to destroy MoS
2interlaminar action, recycling high speed shear emulsification instrument is to the MoS at specific intensive polar solvent
2impose strong shearing force, further destroy MoS
2interlaminar action, finally utilize ultrasonication, will destroy the MoS of interlaminar action
2spread out, under liquid phase state, prepare two-dimentional MoS
2nanometer sheet.
Embodiment two: MoS in the initial mixing liquid that step 1 that what present embodiment was different from embodiment one is obtains
2the concentration of bulk powder is 25mg/mL～125mg/mL.Other step and parameter are identical with embodiment one.
Embodiment three: what present embodiment was different from embodiment one or two is that step 2 adopts high speed shear emulsification instrument, with the shearing rate of 10000rpm～15000rpm, the initial mixing liquid of step 1 is carried out to high speed shear 30min～60min.Other step and parameter are identical with embodiment one or two.
Embodiment four: the supersound process described in step 3 that what present embodiment was different from one of embodiment one to three is is to adopt probe sonication 1h～3h that power is 600W～800W.Other step and parameter are identical with one of embodiment one to three.
Embodiment five: the supersound process described in step 3 that what present embodiment was different from one of embodiment one to three is is to adopt water-bath supersound process 1h～8h that power is 150W～240W.Other step and parameter are identical with one of embodiment one to three.
Embodiment four and five, in the time carrying out supersound process, in order to prevent solvent moisture absorption, can cover on the container that holds solvent with preservative film.
Embodiment six: the mixed solution after the supersound process that step 4 that what present embodiment was different from one of embodiment one to five is obtains step 3 with the rotating speed of 1500rpm～3000rpm carries out centrifugal treating.Other step and parameter are identical with one of embodiment one to five.
Embodiment mono-: the two-dimentional MoS that the present embodiment disperses based on liquid phase
2the preparation method of nanometer sheet follows these steps to implement:
One, by the MoS of the natural hexagonal structure of 4g
2bulk powder is mixed with 40mL1-N-methyl-2-2-pyrrolidone N-(NMP), preparation MoS
2initial mixing liquid;
Two, adopt high speed shear emulsification instrument, with the shearing rate of 10000rpm, the initial mixing liquid of step 1 is carried out to high speed shear 60min, obtain the mixed solution after shearing treatment;
Three, the mixed solution after shearing treatment step 2 being obtained carries out probe sonication 1h with the power of 600W, obtains the mixed solution after supersound process;
Four, the mixed solution after the supersound process with the rotating speed of 1500rpm, step 3 being obtained carries out centrifugal treating, after centrifugal 45min, gets supernatant liquid, leaves standstill 24h, and then gets the supernatant liquid of the reaction solution having left standstill, and obtains two-dimentional MoS
2nanometer sheet suspension.
MoS prepared by the present embodiment
2nanometer sheet suspension is orange-yellow transparent liquid, and nanometer sheet suspension after solvent evaporated, is pale yellow powder in a vacuum.
Fig. 1 and Fig. 2 are MoS prepared by the present embodiment
2moS in nanometer sheet suspension
2the afm image of nanometer sheet and the gauge in cross section.As can be seen from the figure, MoS
2nanometer sheet thickness is about 2nm left and right, and the number of plies is approximately 1～2 layer.
Fig. 3 is the FP-6500 fluorescence spectrophotometer of selecting Japanese JASCO company to produce, the fluorescence spectrum figure recording in the time that excitation wavelength is 514nm, and wherein 1 represents MoS prepared by the present embodiment
2nanometer sheet suspension, 2 represent the MoS that does not carry out high speed shear processing
2nanometer sheet suspension, 3 represent MoS
2bulk powder, 4 represent 1-Methyl-2-Pyrrolidone (NMP).As can be seen from the figure: compare the sample of not shearing, disperse the MoS of preparation through high speed shear
2the fluorescent effect of nanometer sheet suspension is stronger, and intensity has approximately improved 32%, and this shows the MoS preparing by the present invention
2the concentration of nanometer sheet suspension is larger, MoS
2the thickness of nanometer sheet more approaches individual layer.
Embodiment bis-: the two-dimentional MoS that the present embodiment disperses based on liquid phase
2the preparation method of nanometer sheet follows these steps to implement:
One, by the MoS of the natural hexagonal structure of 4g
2bulk powder is mixed with 40ml1-N-methyl-2-2-pyrrolidone N-(NMP), preparation MoS
2initial mixing liquid;
Two, adopt high speed shear emulsification instrument, with the shearing rate of 10000rpm, the initial mixing liquid of step 1 is carried out to high speed shear 30min, obtain the mixed solution after shearing treatment;
Three, the mixed solution after shearing treatment step 2 being obtained carries out water-bath supersound process 1h with the power of 240W, obtains the mixed solution after supersound process;
Four, the mixed solution after the supersound process with the rotating speed of 1500rpm, step 3 being obtained carries out centrifugal treating, after centrifugal 45min, gets supernatant liquid, leaves standstill 24h, and then gets the supernatant liquid of the reaction solution having left standstill, and obtains two-dimentional MoS
2nanometer sheet suspension.
Two-dimentional MoS prepared by the present embodiment
2it is 703 that nanometer sheet suspension records its relative maximum fluorescence intensity in the time that excitation wavelength is 514nm, and the relative maximum fluorescence intensity of comparing the sample of not shearing is 597, and fluorescence intensity has approximately promoted 18%.
Claims (6)
1. a two-dimentional MoS who disperses based on liquid phase
2the preparation method of nanometer sheet, is characterized in that the two-dimentional MoS disperseing based on liquid phase
2the preparation method of nanometer sheet follows these steps to realize:
One, by the MoS of natural hexagonal structure
2bulk powder is mixed with dispersion solvent, preparation MoS
2initial mixing liquid;
Two, adopt high speed shear emulsification instrument, with the shearing rate of 10000rpm～20000rpm, the initial mixing liquid of step 1 is carried out to high speed shear 20min～100min, obtain the mixed solution after shearing treatment;
Three, the mixed solution after shearing treatment step 2 being obtained carries out supersound process, obtains the mixed solution after supersound process;
Four, the mixed solution after the supersound process with the rotating speed of 1500rpm～6000rpm, step 3 being obtained carries out centrifugal treating, after centrifugal completing, gets supernatant liquid, leaves standstill 22～26h, and then gets the supernatant liquid of the reaction solution having left standstill, and obtains two-dimentional MoS
2nanometer sheet suspension;
Wherein the dispersion solvent described in step 1 is 1-Methyl-2-Pyrrolidone, l-vinyl-2-pyrrolidone, dimethyl sulfoxide (DMSO) or dimethyl formamide.
2. a kind of two-dimentional MoS disperseing based on liquid phase according to claim 1
2the preparation method of nanometer sheet, is characterized in that MoS in initial mixing liquid that step 1 obtains
2the concentration of bulk powder is 25mg/mL～125mg/mL.
3. a kind of two-dimentional MoS disperseing based on liquid phase according to claim 1
2the preparation method of nanometer sheet, is characterized in that step 2 adopts high speed shear emulsification instrument, with the shearing rate of 10000rpm～15000rpm, the initial mixing liquid of step 1 is carried out to high speed shear 30min～60min.
4. a kind of two-dimentional MoS disperseing based on liquid phase according to claim 1
2the preparation method of nanometer sheet, is characterized in that the supersound process described in step 3 is to adopt probe sonication 1h～3h that power is 600W～800W.
5. a kind of two-dimentional MoS disperseing based on liquid phase according to claim 1
2the preparation method of nanometer sheet, is characterized in that the supersound process described in step 3 is to adopt water-bath supersound process 1h～8h that power is 150W～240W.
6. a kind of two-dimentional MoS disperseing based on liquid phase according to claim 1
2the preparation method of nanometer sheet, is characterized in that the mixed solution after supersound process that step 4 obtains step 3 with the rotating speed of 1500rpm～3000rpm carries out centrifugal treating.
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Cited By (12)
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| CN104099083A (en) * | 2014-08-06 | 2014-10-15 | 哈尔滨工业大学 | Preparation method of molybdenum compound suspension with photochromic properties |
| CN104140641A (en) * | 2014-08-06 | 2014-11-12 | 哈尔滨工业大学 | Composite material with photochromic performance and preparation method thereof |
| CN104495935A (en) * | 2014-12-03 | 2015-04-08 | 安徽百特新材料科技有限公司 | Preparation method of molybdenum disulfide nanosheet in stripping manner |
| CN104495936A (en) * | 2014-12-12 | 2015-04-08 | 电子科技大学 | Preparation method of stratified molybdenum disulfide nano material |
| CN104667774A (en) * | 2015-02-13 | 2015-06-03 | 中国工程物理研究院机械制造工艺研究所 | Combined type mechanical dispersion method used for nano particle slurry |
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| CN106064833A (en) * | 2016-05-26 | 2016-11-02 | 金堆城钼业股份有限公司 | One is prepared 2H MoS by molybdenum concntrate2the method of nanometer sheet |
| CN106315669A (en) * | 2016-08-30 | 2017-01-11 | 陕西科技大学 | Preparation method of two-dimensional Ti2AlC nanosheets |
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| CN107512735A (en) * | 2017-09-05 | 2017-12-26 | 安阳工学院 | A kind of molybdenum disulfide nano sheet and preparation method thereof |
| CN107555423A (en) * | 2017-08-29 | 2018-01-09 | 北京航空航天大学 | A kind of stripping solution and its application for being used to prepare two-dimension nano materials |
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| CN105039498B (en) * | 2015-06-12 | 2018-11-23 | 青岛科技大学 | A method of the RNA endonuclease activity based on optical diode induced chemical luminescence assays Ago2 albumen |
| CN106064833A (en) * | 2016-05-26 | 2016-11-02 | 金堆城钼业股份有限公司 | One is prepared 2H MoS by molybdenum concntrate2the method of nanometer sheet |
| CN106315669B (en) * | 2016-08-30 | 2017-12-19 | 陕西科技大学 | A kind of two-dimentional Ti2The preparation method of AlC nanometer sheets |
| CN106315669A (en) * | 2016-08-30 | 2017-01-11 | 陕西科技大学 | Preparation method of two-dimensional Ti2AlC nanosheets |
| CN106672954A (en) * | 2017-01-20 | 2017-05-17 | 北京航空航天大学 | Method for preparing graphene two-dimensional material through liquid-phase stripping |
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| CN107512735A (en) * | 2017-09-05 | 2017-12-26 | 安阳工学院 | A kind of molybdenum disulfide nano sheet and preparation method thereof |
| CN109133077A (en) * | 2018-08-14 | 2019-01-04 | 同济大学 | A method of preparing two-dimentional nearly single layer montmorillonite |
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